CN102431966B - Tubular multi-pore micron motor and preparation method and application thereof - Google Patents
Tubular multi-pore micron motor and preparation method and application thereof Download PDFInfo
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- CN102431966B CN102431966B CN201110443627.0A CN201110443627A CN102431966B CN 102431966 B CN102431966 B CN 102431966B CN 201110443627 A CN201110443627 A CN 201110443627A CN 102431966 B CN102431966 B CN 102431966B
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Abstract
The invention belongs to the technical field of micro-nano devices, and in particular relates to a tubular multi-pore micron motor and a preparation method and application thereof. The preparation method of the multi-pore micron motor disclosed by the invention comprises the following steps: carrying out anodic oxidation to prepare an aluminum oxide film the surface of which is provided with a nano-pore array; depositing multiple layers of films having prestress gradient on the anodic aluminum oxide film; carrying out graphical processing on the multiple layers of films; selectively corroding the multi-pore anodic aluminum oxide under the multiple layers of films to cause the multiple layers of films to curl automatically, thus forming a micro tube the wall of which is provided with nano pores; and transferring the multi-pore micro tubes to a solution to obtain a micro motor. The multi-pore micron motor with special structure has large surface area, higher catalytic efficiency and higher movement speed. The moving direction of the micro motor can be controlled by a magnetic filed so as to transport micro-nano level objects. The micro motor moving at high speed has great application prospect in aspects of medicament transportation, biological detection and separation, single-cell analysis and the like.
Description
Technical field
The invention belongs to micro-nano device technical field, be specifically related to a kind of tubular multi-pore micron motor and preparation method thereof and application thereof.
Background technology
Making micron or nano-motor drive and transport micron, sub-micron and nano level object is an important research target of micro-nano device.One of the faced ultimate challenge of realizing this goal be exactly to be made the micro-nano motor with larger power that can high-speed motion.Micro-nano motor generally adopts nano material manufacture, and the energy producing by in-situ chemical reaction provides power.Synthetic and the preparation of traditional nano biological molecular motor is difficulty very, and as the novel micro nanometer motor of driving force, has since two thousand been subjected to the strong interest of scientific circles based on catalytic reaction.The Whitesides of Harvard University in 2002 is usingd oxygen bubble that Pt film catalytic decomposition hydrogenperoxide steam generator produces as motive force, and a centimetre rank floating thing body has been realized to self-propelled and self assembly.Subsequently, Pennsylvania State Univ-Univ Park USA and University of Toronto are applied to this drive pattern on the object of Nano grade, produced and can continue self-propelled various bimetallics (Au/Pt, Au/Ni) nano wire, realized the non-Brownian movement of nanoscale.Arizona, USA university and San Diego, CA university increase the movement velocity of nano-motor by changing the formation of micro-nano motor material and " fuel " solution greatly.Subsequently, the micro-nano motor of some unique design is constantly produced out, as bimetal nano line of the silicon micron ball of asymmetric platinum plating, porous etc.The possibility that adopts micro-nano motor that other micro-nano objects are caught and transported becomes a reality.These catalysis micro-nano motors have huge application potential in fields such as drug delivery, nanometer assembling, cell biology, nanosurgery, the transmission of microfluid object, microrobots.Yet the movement velocity and the power that improve these micro-nano motors remain a urgent problem.
Summary of the invention
The object of the present invention is to provide tubulose micron motor that a kind of driving force is large, movement velocity is fast and its preparation method and application.
Tubulose micron motor provided by the invention, its tube wall has high density nano-pore, thereby has high surface area, and high catalytic efficiency.
Tubular multi-pore micron motor provided by the invention, its preparation method comprises following step (seeing accompanying drawing 1):
(1) adopt anode oxidation method preparation table mask to have the periodically multiaperture pellumina of nanohole array of high density, in order to as sacrifice layer template;
(2) adopt physical gas-phase deposite method on multiaperture pellumina, to deposit the plural layers with prestressing force gradient; Described internal stress gradient comes from different thermal coefficient of expansion between plural layers different layers and different growth rates; In described plural layers, having the material of thin film is the magnetic materials such as iron, cobalt or nickel, and the material of the superiors' film is catalysis material, and the material of all the other each layer films can be identical, also can be different;
(3) adopt diamant that the plural layers on Woelm Alumina are divided into square that size is 10-2000 μ m size;
(4) optionally remove porous oxidation aluminum sacrificial layer, upper strata square multi-layer film is from being rolled into micron tubular structure, and its tube wall is cellular;
(5) resulting multi-pore micron pipe is transferred in solution, the catalytic material catalyzes solution of micron tube inwall decomposes generation gas and forms micron bubble, and bubble is discharged from multi-pore micron pipe end, and the anti-micron tube that pushes away travels forward, and becomes a micron motor.
The direction of motion of above-mentioned tubulose micron motor can utilize magnetic field to control, and object transport is arrived to specified position.
In the present invention, the geometric parameter of resulting tubular multi-pore micron motor, as tube wall nano-pore diameter, the spacing between Kong Yukong and micron tube diameter etc., determine according to designing requirement.
In the present invention, when step (1) adopts anodic oxidation to prepare multiaperture pellumina, can be by taking different electrolyte as phosphoric acid, oxalic acid or sulfuric acid, and take different decomposition voltages and time, obtain different nano apertures, and can modulate the spacing between Kong Yukong.Modulation can be carried out in the aperture of nano-pore within the scope of 20-200 nm.
In the present invention, the film deposition process of step (2) can form prestressing force gradient in film, thereby realizes final from curling.The large I of prestressing force gradient regulates by the deposition parameter of controlling in processes of physical vapor deposition.These deposition parameters comprise: deposit thickness is controlled as 5-100 nm, and sedimentation rate is controlled as 0.2-20/s, and underlayer temperature is controlled as 25-300
oc, and the control of deposition pressure is 10
-3-10
-4pa.Wherein, the method for physical vapour deposition (PVD) comprises magnetron sputtering, thermal evaporation, or electron beam evaporation etc.
In the present invention, the plural layers that deposit on multiaperture pellumina can be the combinations of a kind of material or different materials.In plural layers, the superiors are necessary for catalyst material, and it is the magnetic materials such as iron, cobalt or nickel that must there be one deck in intermediate layer.The diameter of multi-pore micron pipe can be carried out modulation in 1-100 μ m scope.
In the present invention, described catalysis material can be Pt or Ag.
In the present invention, the described solution of step (5) is to be decomposed the solution that produces gas by described catalysis material, as rare H
2o
2.
In the present invention, described sacrifice layer and template are porous anodic aluminium oxide.
In the present invention, in the deposition process of step (2), owing to being deposited material, can enter alumina nanohole, after final pellumina is corroded, the material that enters alumina nanohole forms nano tube structure.Thereby for the tubulose micron motor of equal length and diameter, multi-pore micron motor, than the smooth micron motor of tube wall, has higher surface area, can improve catalytic efficiency.
In the present invention, multi-pore micron motor adopts liquid fuel, realizes self-driven in liquid.
In the present invention, multi-pore micron motor, than the smooth micron motor of tube wall, has movement velocity faster.Its concrete validate mode is as follows:
Adopt the motion of observation by light microscope micron motor in solution, and its motion is recorded a video, then can carry out analysis and calculation to the motion video recording of the micron motor of taking.Movement velocity to the multi-pore micron motor of a plurality of certain lengths and diameter in a certain solution is added up, and calculates its average speed.Meanwhile, make the smooth micron motor of tube wall of equal length and diameter, add up the movement velocity of a plurality of smooth micron motors in the solution of same concentrations, and calculate its average speed.More above-mentioned two average speeds, just can know that multi-pore micron motor can obtain great acceleration.
The multi-pore micron motor of this special construction has large surface area, higher catalytic efficiency and movement velocity faster; Utilize magnetic field to control transporting for micro-nano rank object to the direction of motion of micron motor.This high-speed motion micron motor has huge application prospect in drug delivery, biological detection with aspects such as separated, single cell analysis.
Accompanying drawing explanation
Fig. 1 is the flow chart that the present invention prepares multi-pore micron motor.Wherein, (a) be fine aluminium sheet; (b) porous anodic alumina template that expression forms by anodic oxidation; (c) represent to utilize physical gas-phase deposite method in template, to prepare the plural layers with prestressing force gradient, be deposited material and can deposit and enter nano-pore one segment distance; (d) represent porous anodic aluminium oxide sacrifice layer to remove, upper strata plural layers are from the curling multi-pore micron pipe that becomes.
Fig. 2 is multi-pore micron pipe schematic diagram as the motion of micron motor in hydrogen peroxide.
Fig. 3 is the schematic diagram of multi-pore micron motor catalytic reaction mass transport process.
Fig. 4 is the electron micrograph of multi-pore micron motor (tube wall nano aperture is 50 nm).
Fig. 5 is A) smooth micron motor, B) tube wall nano aperture is the multi-pore micron motor of 50 nm, C) tube wall nano aperture is that the multi-pore micron motor of 200 nm is the average speed comparison of moving in the hydrogen peroxide solution of 7 % in concentration.The statistic bias of mean value is corresponding marking also.
Fig. 6 is for adopting multi-pore micron motor to carry out the schematic diagram of the object transport of micron level.
Number in the figure: 1. fine aluminium substrate, 2. anode multiaperture pellumina, 3. multiple layer metal film, 4. multi-pore micron motor, the 5. nanotube (hole) of micron motor tube wall, 6. oxygen micron bubble, 7. object to be transported.
The specific embodiment
Below in conjunction with accompanying drawing and instantiation, to preparing multi-pore micron pipe and high-speed motion, object, transport application and be described further.
Fig. 1 utilizes method of the present invention to prepare the schematic diagram of multi-pore micron pipe.Wherein, (a) be pure aluminium flake 1.(b) represent, the ordered porous alumina 2 that utilizes anodic oxidation to form, it is simultaneously as the sacrifice layer in curly course.The geometry of the nanohole array on anodised aluminium surface can be controlled by anodised bath composition concentration and voltage.(c) show to adopt method deposit multilayer metallic film 3 on porous anodic alumina films of physical vapour deposition (PVD), the superiors are platinum film, in order to catalysis decomposing hydrogen dioxide solution.Can, by changing deposition parameter, as deposit thickness, sedimentation rate, underlayer temperature and deposition pressure etc., the caliber of final curling tubulose micron motor be controlled.(d) utilizing mass percent is that the potassium hydroxide solution of 20 % is removed porous anodic aluminium oxide sacrifice layer, and d/d multiple layer metal film is from the curling multi-pore micron pipe 5 that becomes.
Fig. 2 illustrates multi-pore micron pipe catalysis decomposing hydrogen dioxide solution in hydrogen peroxide solution to produce the process of bubble motion, and the bubble producing in micron tube can spray from one end of micron tube, thereby promotes micron tube counter motion.
Fig. 3 illustrates the mass transport process of multi-pore micron motor catalysis decomposing hydrogen dioxide solution, and due to the existence of tube wall nano-pore, hydrogen peroxide can enter tube chamber from nano-pore, by the platinum catalytic decomposition of lumen wall.Greatly accelerate the decomposition rate of hydrogen peroxide, thereby accelerated the speed of micron motor.
embodiment 1
Wherein, described porous anodic alumina films is in the oxalic acid solution of 0.5 M, to add 40 V voltages pure aluminium flake is carried out to anodic oxidation to obtain, and its pore size is in 50 nm left and right, and hole density is ~ 10
14m
-2.
On multiaperture pellumina, deposit multiple layer metal film be respectively from top to bottom titanium, chromium, cobalt, platinum, thickness is respectively 5 nm, 5 nm, 5 nm, 5 nm.Processes of physical vapor deposition adopts electron-beam evaporation mode, and sedimentation rate is 0.5/s respectively.
Adopt diamant to carry out horizontal and vertical scribing to the metallic film of above-mentioned Woelm Alumina surface deposition, the square area of gained is 20 * 20 μ m
2.
The corrosion process of described Woelm Alumina is that above-mentioned sample is put into the potassium hydroxide solution that mass percent is 20 %.D/d metal multilayer film is curling becomes the tubular structure that diameter is 3.8 μ m, and wherein on tube wall, the diameter in the hole of periodic arrangement is less than the aperture on porous anodic alumina template, is about 20 nm, as shown in electron micrograph in accompanying drawing 4.
The degree of depth that multiple layer metal enters nano-pore in electron-beam evaporation process is about 200 nm, and the multi-pore micron tube-surface porous place connecting length finally obtaining is the nanotube of 200 nm left and right, as shown in electron micrograph in accompanying drawing 4.
Described multi-pore micron pipe obtains 3.9 times of surface area that surface area is the smooth micron tube of equal length and diameter.
Described multi-pore micron motor is put in the hydrogen peroxide solution of 7 %, the platinum catalysis hydrogen peroxide solution decomposition of micron tube inwall produces oxygen and forms micron bubble, bubble is discharged from multi-pore micron pipe end, and the anti-micron tube that pushes away travels forward, and becomes a micron motor (accompanying drawing 2).Loose structure has been accelerated decomposing hydrogen dioxide solution, thereby has accelerated the movement velocity (accompanying drawing 3) of tubulose porous motor.
Adopt light microscope to take its motion video recording and carry out analytical calculation, finally the speed of 20 multi-pore micron motors add up that to obtain average speed be that 613 μ m/s(are shown in B in accompanying drawing 5), be 2.3 times (seeing A in accompanying drawing 5) of the smooth micron of motor speed of tube wall of same diameter and length.
embodiment 2
Wherein, described porous anodic alumina films is in mass fraction is the phosphoric acid of 6 %, to add 80 V voltages pure aluminium flake is carried out to anodic oxidation to obtain, and its pore size is in 200 nm left and right, and hole density is ~ 4 * 10
13m
-2.
The multiple layer metal film depositing on multiaperture pellumina is respectively titanium, chromium, cobalt, platinum from top to bottom, and thickness is respectively 5 nm, 5 nm, 5 nm, 5 nm.Processes of physical vapor deposition adopts electron-beam evaporation mode, and sedimentation rate is 0.5/s respectively.
Adopt diamant to carry out horizontal and vertical scribing to the metallic film of above-mentioned Woelm Alumina surface deposition, the square area of gained is 20 * 20 μ m
2.
The corrosion process of described Woelm Alumina is that above-mentioned sample is put into the potassium hydroxide solution that mass percent is 20 %.D/d metal multilayer film is curling becomes the tubular structure that diameter is 3.8 μ m, and wherein on tube wall, the diameter in the hole of periodic arrangement is close with the aperture on porous anodic alumina template but smaller, is about 180 nm.
The degree of depth that multiple layer metal enters nano-pore in electron-beam evaporation process is about 500 nm, and the multi-pore micron tube-surface porous place connecting length finally obtaining is the nanotube of 500 nm left and right.
Described multi-pore micron pipe obtains 9.7 times of surface area that surface area is the smooth micron tube of equal length and diameter.
Described multi-pore micron motor is put in the hydrogen peroxide solution of 7 %, adopt light microscope to take its motion video recording and carry out analytical calculation, finally the speed of 20 multi-pore micron motors add up that to obtain average speed be that 1077 μ m/s(are shown in C in accompanying drawing 5), be 4.1 times (seeing A in accompanying drawing 5) of the smooth micron of motor speed of tube wall of same diameter and length.
embodiment 3
Wherein, similar front embodiment 2, prepares pipe diameter size and is about 3.8 μ m, and tube wall nano-pore diameter is about the tubulose loose structure of 200 nm.
Described tubulose loose structure is positioned in the hydrogen peroxide solution of 7 %, forms tubular multi-pore micron motor.
Adopt externally-applied magnetic field to control the motion of micron motor, the direction of motion and the magnetic direction of micron motor are consistent, and can to the motion of micron motor, control very easily.
In above-mentioned solution, place 50 * 50 * 10 μ m
3square, utilizes magnetic field to control the motion of micron motor, and it is carried square.Under the controlling in magnetic field, micron motor can find the square of required carrying accurately, and promotes the direction motion (accompanying drawing 6) that it is controlled according to magnetic field.
In described freight handling process, the speed of micron motor is by drop to ~ 150 μ m/s of ~ 1200 μ m/s.
Claims (8)
1. a preparation method for tubular multi-pore micron motor, is characterized in that concrete steps are:
(1) adopt anode oxidation method preparation table mask to have the periodically multiaperture pellumina of nanohole array of high density, in order to as sacrifice layer template;
(2) adopt physical gas-phase deposite method on multiaperture pellumina, to deposit the plural layers with prestressing force gradient; Described prestressing force gradient comes from different thermal coefficient of expansion between plural layers different layers and different growth rates; In described plural layers, the material that has thin film is iron, cobalt or nickel magnetic material, and the material of the superiors' film is catalysis material, and the material of all the other each layer films is identical, or different;
(3) adopt diamant that the plural layers on Woelm Alumina are divided into square that size is 10-2000 μ m size;
(4) optionally remove porous oxidation aluminum sacrificial layer, upper strata square multi-layer film is from being rolled into micron tubular structure, and its tube wall is cellular;
(5) resulting multi-pore micron pipe is transferred in solution, the catalytic material catalyzes solution of micron tube inwall decomposes generation gas and forms micron bubble, and bubble is discharged from multi-pore micron pipe end, and the anti-micron tube that pushes away travels forward, and becomes tubular multi-pore micron motor.
2. preparation method according to claim 1, the aperture that it is characterized in that multiaperture pellumina described in step (1) is 20-200 nm.
3. preparation method according to claim 1, is characterized in that described catalysis material is Pt or Ag.
4. preparation method according to claim 1, is characterized in that in step (2) processes of physical vapor deposition, controlling deposition parameter is: deposit thickness 5-100 nm, sedimentation rate 0.2-20/s, underlayer temperature 25-300
oc, deposition pressure 10
-3-10
-4pa.
5. preparation method according to claim 3, is characterized in that in step (4), multi-pore micron pipe diameter is 1-100 μ m.
6. the tubular multi-pore micron motor that method prepares as described in one of claim 1-4.
7. tubular multi-pore micron motor as claimed in claim 6, is characterized in that the motion of this motor is controlled by magnetic field.
8. the application of tubular multi-pore micron motor as claimed in claim 6 aspect drug delivery, biological detection and separated, single cell analysis.
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| CN101716529A (en) * | 2009-12-11 | 2010-06-02 | 北京工业大学 | Method for preparing high-loading catalyst Pt/CNTs |
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| US20050276743A1 (en) * | 2004-01-13 | 2005-12-15 | Jeff Lacombe | Method for fabrication of porous metal templates and growth of carbon nanotubes and utilization thereof |
| KR100747074B1 (en) * | 2006-10-25 | 2007-08-07 | 금오공과대학교 산학협력단 | Method for fabricating the nanorod by aao template and the nanorod using the method |
| WO2011031463A2 (en) * | 2009-08-25 | 2011-03-17 | The Regents Of The University Of California | Nanomotor-based patterning of surface microstructures |
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